CN1675530A - Method and apparatus for pumping and diluting a sample - Google Patents
Method and apparatus for pumping and diluting a sample Download PDFInfo
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- CN1675530A CN1675530A CN03819412.0A CN03819412A CN1675530A CN 1675530 A CN1675530 A CN 1675530A CN 03819412 A CN03819412 A CN 03819412A CN 1675530 A CN1675530 A CN 1675530A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1095—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
- G01N35/1097—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers characterised by the valves
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
Abstract
A pumping apparatus ( 50 ) which isolates a sample ( 52 ) from a pump ( 72 ), thereby circumventing the so-called 'memory effect' problem. The sample is pumped into an intermediary, or buffer region ( 64 ) using a first pump ( 54 ). The sample is displaced from this buffer region by pumping a second fluid ( 74 ) into the buffer region using a second pump ( 72 ). When the sample is displaced from the buffer region it proceeds to a mixer ( 78 ) where it can be diluted before analysis. The second pump is required to operate with a high degree of accuracy so that the sample is diluted by a consistent amount. Preferably, the second pump is a highly accurate piston pump.
Description
Technical field
The present invention relates to a kind ofly be used for that sample is drawn into analytical equipment and this sample of dilution or be used for the method and apparatus of any other reason before analyzing this sample.
In this article, with reference to needing diluted liquid-like to describe the present invention originally before in mass spectrometer, being analyzed.Yet, the invention is not restricted to liquid sample or mass spectrophotometry, and the present invention sample and any other test or analytical equipment that can be applicable to equally dissolve or that suspend.
Background technology
Be used for analyzing liquid TRACE ELEMENTS ANALYSIS equipment to dissolved solid material or matrix (such as CaCO
3Or being dissolved in salt or its analog in the water) measurement capability of the higher sample of content is limited.The trace element that the user was concerned about only accounts for parts per billion or still less usually, and matrix can account for 1,000,000 parts several or higher.So the matrix of high-load can cause harmful effect to analytical equipment, and for example, material can be deposited on spray orifice, glassware and the ion optical element.Therefore, be necessary diluted sample before analysis.
Inductively coupled plasma mass spectrometry instrument (ICP-MS) requires total dissolved solidss content less than 2000mg/l usually, to avoid these adverse influences.The solid of dissolving can be deposited on the assembly in the instrument, for example is deposited in order to the sampling plasma and skims on the cone of a part of choked jet, thereby significantly reduce test result and any result's that other is tested subsequently reliability.If the material deposition has taken place, must after cleaning instrument up hill and dale, just can restart accurate test so.
Test laboratory needs the many samples of express-analysis usually, and wherein the matrix content of each sample alters a great deal.Usually, the user will wish that predetermined amounts dilutes each sample and whether can just can be analyzed without dilution with analyte and this sample that judgement is present in each sample.Dilution if desired, this initial testing can provide the indication to dilution gfactor so, and it is required that described dilution gfactor makes total dissolved solidss content reduce to the acceptable level of instrument.
If there are every day many samples to need to analyze, these manual interventions are with regard to hell to pay so, and are too consuming time and cost is too high.At present, in case cleaned analyzer, just reanalyse the sample that can cause unaffordable dissolved solid burden to instrument.Must to stop to analyze in order cleaning, and must to reanalyse at the analyzed sample in the contaminated back of analyzer owing to neglect.This just needs considerable operator intervention.This quantitative limitation is that we are reluctant to see to sample process, and operator intervention is with high costs.
Used dilution system automatically in the past, referring to Fig. 1, it has shown a kind of like this automatic system 10 as known in the art with highly graphic form.Sample pump 14 is drawn into mixing tube 16 with sample 12 from container.Similarly, diluent pump 20 is drawn into mixing tube 16 with thinning agent 18 from independent thinner container.Described sample mixes fully with thinning agent in mixing tube and is diluted.The sample that instrument pump 22 will be diluted is drawn into from mixing tube in instrument or the analyzer and (does not show among Fig. 1).
Sample pump and diluent pump all must be able to keep accurate flow rate to guarantee accurately diluted sample.If dilution does not remain on the known level and do not remain within the strict relatively tolerance, the precision of analysis result may be unacceptable so.Equally, instrument flow must remain on accurate flow rate, to guarantee to be drawn into the sample that known controllable speed will be diluted the input end of analyzer.Thereby all pumps (with their associated flow rates) need be subjected to accurately control to keep accurate test result.
At present, use peristaltic pump to come the sample after aspiration sample, thinning agent and the dilution to pass through dilution system.Usually 50: 1 thinning agent is used for mass spectrophotometry to the dilution ratio of sample.Therefore, diluent pump rate is bigger 50 times than sample pump speed usually.The flow rate of peristaltic pump be limited in scope and sample pump and diluent pump usually with the ultimate value work of its flow rate range.Equally, the limited flow rate restrictions of peristaltic pump can be used to the dilution gfactor of diluted sample; Maximum dilution when working with minimal flow speed with maximum flow rates work and sample pump, diluent pump takes place.
The speed that should have when the sample that diluted enters the instrument (not shown) depends on the type of used instrument, but this speed is relatively low and be generally several milliliters of per minutes.If surpass this speed, instrument stops up the sample of diluted mistake, and this will throw into question in mass spectrometer and analysis result is had harmful effect.Usually, the combination flow rate of sample pump and diluent pump is considerably beyond the flow rate of instrument pump.This be because all pumps all have similar relatively flow rate range, and for example dilution gfactor greater than 10 situation under, diluent pump 20 must be with high flow rate work.This high flow rate surpasses the acceptable flow rate of analytical instrument usually.Therefore, need provide waste liquid outlet 24 to prevent the accumulation of pressure in system; The sample that is not drawn into the excessive dilution in the instrument flows to waste fluid container 26.Under the situation of the highly diluted factor, the comparable flow that enters in the instrument of solution that flows to waste fluid container is high 50 times.Material in the waste fluid container is dropped; Because the accurate needed high quality diluent of test result is relatively costly, so this kind loss is the extra financial burden of test laboratory.
Shown another kind of auto-pumping as known in the art system 28 with highly graphic form among Fig. 2.Syringe pump 31 along first conduit, 30 aspiration sample 29 with the filled syringe (not shown).Valve-off 32 is in case the fluid stopping body enters syringe from pump release catheter 33.When pump is filled the sample of appropriate amount, open valve and with constant speed pulling syringe embolism, so that the sample flow along conduit 33 by direction shown in the arrow Z to be provided roughly.One-way cock (not shown) in the pump prevents that sample from flowing back to container 29 in the stage of flowing along conduit 33.
Defined the Mixed Zone 34 of this conduit with second conduit 35 of the structure that is roughly " T " or " Y " shape and conduit 33 adjacency.When instrument pump system (for example, sprayer) suction solution, can produce uncontrolled pressure in the conduit 35 and descend.This can cause solution 34 to flow along conduit 33 ' from the Mixed Zone uncontrollably.This flow rate is from the in check flow of solution of syringe pump and the combination of flowing along the uncontrolled thinning agent of conduit 35.If flowing of uncontrollable thinning agent will cause uncontrollable dilution gfactor.In this configuration, there is not instrument pump that the sample that diluted is drawn into analyzer.
Rely on the system of this configuration to go wrong.For example, the available dilution gfactor of this system is conditional, particularly when analyzer need aspirate the sample that diluted with special speed.Can be similar to the instrument pump and the pressure release system that show among Fig. 1 and overcome this problem by providing.Yet the problem (for example, thinning agent discarded object) relevant with system among Fig. 1 becomes generally in this system now.
At US 4,245, disclosed suction system as known in the art among 509 (instrument experiment chamber company limited (InstrumentationLaboratory Inc.)) and the US 5,007,297 (Pacific Scientific Company (PacificScientific Company)).
In addition, the pollution that is exposed to the pump parts of sample during operation can cause sample subsequently contaminated, thereby causes coarse analysis result.This so-called " memory effect " problem bothers especially to the hypersensitivity analytical instrument.Along with testing tool becomes more responsive, this problem is more remarkable.(for example, we have found that this problem is very little to the influence of analysis result when the atomic absorption analyzer device that uses relative insensitivity comes test sample book, but when using hypersensitivity ICP-MS analysis tool to come test sample book, this problem will be difficult to handle.)
Equally, but some fluid damage pump components.These assemblies that are damaged can cause coarse flow rate, or even more serious, and they can make pump become unavailable under the situation of time-based maintenance not repairing for a long time or do not have.
Use peristaltic pump at present; The liquid that is sucked only contacts with conduit (it can be made by resilient material) in these pumps.Yet as previously mentioned, peristaltic pump does not have enough flow rate range and enough accuracies distribute sample solution with enough low flow rate, to avoid useful release of fluid in waste fluid container.In addition, because the limited effective flow rate range of peristaltic pump uses peristaltic pump can limit accessible dilution gfactor.
Summary of the invention
An object of the present invention is to improve the problem relevant with prior art.
Or rather, the invention provides and a kind of sample is drawn into analyzer for the pumping unit of analyzing, this equipment comprises: first pump, and it is configured to first flow rate sample be aspirated in the buffer area; With second pump, it is configured to subsequently with second flow rate second fluid to be aspirated in this buffer area, to impel at least a portion sample, can operate this second pump so that second flow rate is compared first flow rate and can be subjected to more accurate control from cushioning zone-transfer to analyzer.
Advantageously, second fluid is aspirated into second pumping unit and the sample isolation of buffer area, so that this pumping unit does not contact with sample and therefore overcome the memory effect problem.In addition, because can control the flow rate of second pump with high relatively degree of accuracy, so the dilution of sample subsequently can reach higher level, and this for the influence system compared to existing technology of analysis result still less, and we find that this is necessary for accurate relatively analytical equipment (for example ICP-MS).
Embodiments of the invention also can comprise the fluid flow switch device that can move between the primary importance and the second place, like this configuration this fluid flow switch device so that: (a) when this switchgear is arranged in primary importance, the buffer area is communicated with the second pump fluid, (b) when this switchgear is arranged in the second place, the first buffer area port is communicated with outlet conduit, and the second buffer area port is communicated with the first pump fluid.
Embodiments of the invention also can comprise a waste solution channel, dispose this waste solution channel like this so that: when this switchgear was arranged in primary importance, the buffer area also was communicated with the waste solution channel fluid.
Embodiments of the invention can comprise that also when this switchgear was arranged in the second place, waste solution channel was communicated with the second pump fluid, and this second pump can be configured to aspirate irrigation.
Embodiments of the invention can further comprise,
When this switchgear was arranged in primary importance, first pump was communicated with the outlet conduit fluid, so that second fluid is drawn in the outlet conduit, to shift the sample fluid or second fluid wherein.
Advantageously, embodiment further comprises the 3rd pumping unit that is used for the Mixed Zone of sample and mixing diluents and the sample that is used for will diluting from this Mixed Zone are drawn into analyzer, and wherein, this Mixed Zone places between outlet conduit and the analyzer.
The present invention further provides a kind of suction system that uses the sample fluid that is used to analyze is drawn into the method for analytical instrument, this suction system comprises: the buffer area of storing sample fluid, and this buffer area is configured to have at least two ports; This method comprises: use first pumping unit by first port second fluid to be drawn in the sample fluid buffer area, by this sample fluid in the described buffer area is transferred in the analyzer.
Advantageously, further comprise second pumping unit and during the outlet conduit that is configured to flow for sample fluid and/or the fluid in analyzer, this method also can comprise uses second pumping unit that sample is drawn in the buffer area when this system.
Advantageously, when this system further comprises the fluid flow switch device that can move between the primary importance and the second place, this method further provides: when this fluid flow switch device is arranged in primary importance, use second pump that sample is drawn in the impact damper, this fluid flow switch device is switched to second place place, and use first pump that second fluid is drawn in the buffer area to shift the sample in the described buffer area; Wherein this fluid flow switch device disposed like this so that: (a) when this switchgear is arranged in primary importance, the buffer area is communicated with the second pump fluid, (b) when this switchgear is arranged in the second place, the first buffer area port is communicated with outlet conduit, and the second buffer area port is communicated with the first pump fluid;
The present invention further also provides a kind of first pumping unit that prevents by the method for sample contamination, this method comprises: use second pump that sample is placed zone line, by using first pumping unit that second fluid is drawn in this zone line, so that sample is migrated out from this zone line.
Main advantage of the present invention roughly is a kind of suction or dilution system, with the flow rate that is determined by the high precision pump sample is drawn in the analytical instrument in this system, and does not make this pump be exposed to sample.The possibility that this can reduce the sample damage or pollute this pump.Equally, the relative high precision dilution of sample may need accurate flow rate.
Being also advantageous in that of embodiments of the invention provides and has been easier to control and the better a kind of suction/dilution system of accurate level and the method for flow rate and dilution gfactor.Equally, in fact do not waste any thinning agent in normal work period.Can advantageously use controller to control the flow rate of the second and the 3rd pump.Can control a dilution gfactor easily by the flow rate of correspondingly adjusting second pump and/or the 3rd pump, this dilution gfactor equals the ratio of the 4th flow rate to second flow rate.Can respond substantially from the data of analytical equipment the control of dilution gfactor and to take place in real time.Equally, be used for providing pump assembly accurate, low-level sample flow can not be exposed to latent lesion corrosion thing, chemical corrosion or the wearing and tearing that solid caused that suspend by sample.Sample solution can not enter second pump.
The further advantage of embodiments of the invention is for having reduced operator intervention in a large number and having increased sample throughput rate.These embodiment purposes are: before introducing sample in the analyzer, provide stable and safe sample dilutes automatically.Sample throughput rate can obtain very big increase.Sample is diluted to being also advantageous in that of security level: come in sample, on minor levels, to carry out analysis with required precision by automatic dilution to sample.Also can introduce new (or different) sample solution apace in impact damper relatively, thereby increase the treatment capacity of sample by the flow rate in the absorption of control sample.Can reduce the cost of diluted sample by the amount that reduces the used thinning agent of dilution system; May only can consume sample is diluted to the needed dilution dosage of required security level, and seldom or do not have thinning agent to be wasted." security level " refers to avoid the necessary dilution gfactor of contamination analysis instrument.
Description of drawings
Now with reference to the accompanying drawings, one embodiment of the present of invention are described by example, wherein:
Fig. 1 is the synoptic diagram of known and aforesaid a kind of pumping system in this area;
Fig. 2 is the synoptic diagram of known and aforesaid a kind of pumping system in this area;
Fig. 3 is a kind of synoptic diagram of realizing pumping system of the present invention, and this system has a switch in primary importance; With
Fig. 4 is the synoptic diagram of switch in the second place of Fig. 3.
Embodiment
With reference to figure 3, it shows that with schematic form is realized a pumping system 50 of the present invention.Analyzed sample 52 is drawn into a valve or conduit fluid flow switch 58 by self-actuated sampler 54 from container along first conduit or sample draw catheter 56.The self-actuated sampler that uses among this embodiment is known by the people in the art and it comprises a pump (not shown) and a probe 60.This probe can be moved and insert the fluid that is arranged in the container under this probe.Different containers can be placed on the carrousel (not shown), so that can with the self-actuated sampler pump different samples or clean-out system 62 be drawn in the pumping system by probe.
In initial or sample suction phase, when sample being drawn in this system, dispose this switch (primary importance) as shown in Figure 3 like that, port F, port B are connected to port C and port D is connected to port E so that port A is connected to.Thereby fluid can be connected to port A and F respectively, port B and C, and flow between the conduit of port D and E.
Second conduit or sample storage conduit 64 connectivity port E and port B.Thereby, in the sample suction phase, extract sample out switch port E and sample be drawn in second conduit 64 by switch port D; Described port is carried out action and is flowed through port to allow fluid, and flows to or flow out conduit, pipeline or the chamber that links to each other with this port.Enter in second conduit sample can by port B with any fluid transfer that has existed in second conduit in switch.The 3rd conduit or waste solution channel 66 are connected to the port C (this port C is connected to port B again in the sample suction phase) and the waste liquid unit 68 of switch.Like this, the fluid that is shifted out from the second conduit transfer is pushed through switch (by port B and C), enters discharge opeing or waste liquid unit along the 3rd conduit.
Now will describe the second sample suction stage of pumping system, in this stage, sample will be drawn in the instrument for analysis.In case second conduit 64 has been full of enough samples, self-actuated sampler just stops from the container aspiration sample.Switch is switched to the second place place shown in Fig. 4, be connected to port B at second place middle port A, port C is connected to port D, and port E is connected to port F.This construction of switch is connected to second a supravasal end by switch port A and B with the 4th conduit or systems pumps conduit 70 now.Second conduit is connected to the end of port B away from self-actuated sampler, and the fluid in this conduit leads to waste liquid outlet (as described previously) by this end.Like this, because second conduit all has been full of sample, this end holds sample fluid.
Can operate first systems pumps 72 now is drawn into fluid or thinning agent 73 the port A from container 74.This fluid preferably is suitable for diluted sample and should has the purity of high level.Fluid is drawn in the switch (port A) by pump 72, and is sucked into thus in the far-end (port B) of second conduit.By this way, the sample in second conduit 64 is migrated out from second conduit, by switch port E, flows out switch port F, and shifts the 5th conduit or switch delivery channel 76.Equal along the flow rate of the pump fluid of the 4th conduit 70 along the flow rate of the 5th conduit (rise/minute).Certainly, this be at the incompressible and conduit of supposition fluid under the non-bloating situation of normal work period.
Simultaneously, switch the sampler probe now, so that via port D, E, B and C another fluid 62 is drawn in the conduit 56 by switch 58 and along second conduit 66.Another fluid preferably is suitable for cleaning or go out the sample fluid in conduit 56 and the probe, thereby cleans these assemblies in the waste fluid container 68 by sample solution is flushed to by conduit 66, thus for sampling next time ready.Present first conduit is communicated with (because this switch be in the second place) by switch port D and C with the 3rd conduit 66, so that washing fluid pours sample waste liquid conduit 66 and is flushed to the liquid waste treating apparatus 68 from conduit 56.
The flow rate of the sample by the 5th conduit 76 is controlled to be flow velocity 1 by sample pump 72.Sample enters the Mixed Zone 78 of the 5th end of conduit, mixes with thinning agent 80 there.78 places in the Mixed Zone, the 5th conduit 76 engages with the 6th conduit or sample diluent conduit 82 and forms single the 7th conduit or instrument input pipe 84.This mixer is the joint of " Y " or "T"-shaped structure in pipeline or the conduit.Also can use more complicated shape or structure to promote mixing of sample and diluent solution.The outlet of Mixed Zone comprises single conduit 84, and described conduit 84 is arranged between the Mixed Zone and second pump 86, and this second pump 86 is drawn into fluid the instrument (not shown) for analysis from the mixed zone.
The mixed process of sample and thinning agent occurs in the interface place of the 5th, the 6th and the 7th conduit 76,82 and 84 respectively, and this mixed process is in order to form the sample that diluted.Extra mixed process also can take place along the certain-length of the 7th conduit (not shown) from the mixer to the analyzer, but mixed process should be finished before the sample that diluted enters analyzer.At joint with under the turbulent flow of the 5th conduit place sample and thinning agent, and also mix owing to the diffusion of these two kinds of fluids.In this embodiment, mixing also can be along with fluid takes place through second pump 86.
First pump or sample pump 72 are preferably the piston-type pump of the milliGAT pumping head that is similar to global FIA company limited (Global FIAInc.) and supplied (be disclosed in US 6,079,313 in).This pump is compared peristaltic pump can allow much bigger flow rate range (for example), and if desired, this pump can aspirate the sample of few relatively volume continuously with flow rate constant or that change in operation.Especially, this pump can be carried low-down flow rate with high-caliber accuracy and accuracy.In addition, this piston pump system does not have the previous relevant shortcoming of pumping system described and prior art.Second pump or instrument pump and first pump can be same type, and perhaps (if suitable) can be peristaltic pump.
Usually, self-actuated sampler also is a peristaltic pump.The advantage that this pump is used for the sample suction is: sample can be remained on the pump line road, thereby sample can not damage any pump assembly.Yet peristaltic pump can not be with needed degree of accuracy and to be close to the pulseless fluid that distributes low rate (being generally several microlitres of per minute) that transports.Therefore peristaltic pump only limits to high relatively rate of volume flow (several milliliters of per minutes), and the relative out of true of aspiration rate, inaccurate.These peristaltic pumps are suitable for application described herein, and sample storage can be filled very soon in this application, and pump is not corroded or the puzzlement of mechanical damage.Certainly, these pumps are not suitable for sample is drawn into mixer 78, because they do not have the controllability of same amount in the flow rate that keeps the required unanimity of accurate sample dilution gfactor.In other words, the flow rate of these unaccommodated pumps can change or pulse, and its variation or degree of pulsatility may work the mischief to the consistance of the sample that diluted.
Flow velocity 1+ flow velocity 2=flow velocity 3;
Suppose that the liquid in the conduit is incompressible.(can to rise/minute be that this flow velocity is measured by unit).
Preferably keep flow velocity 3 constant, so the arrival rate of the sample of the dilution of instrument can be constant by second pump 86.Therefore, the flow rate that changes first pump can change the dilution gfactor D of diluted sample, wherein
D=flow velocity 2/ flow velocity 1, or
D=(flow velocity 3/ flow velocity 1)-1.
So, be constant according to above equation and supposition flow velocity 3, the reduction of the flow rate of first pump (flow velocity 1) can increase the thinning agent that flows to the mixer district flows, and therefore can increase dilution gfactor D.
An example realizing that how pumping system of the present invention works with the ICP-MS instrument is provided now.During operation, can be before analyzing samples by discrete dilution gfactor D
1Dilute all samples routinely.At first with D
1Be set at high relatively level, so that when analyzing samples, the degree that the diluted arrival of sample is such, promptly any dissolved solid (or matrix) in the sample all is able to abundant dilution.By this way, can prevent or reduce adverse effect to analytical instrument or test result.Usually, D
1=100.
Judge the degree that the sample mesostroma dilutes by the analysis software of checking analyser results, need to determine whether further dilution.And, the degree of accuracy of the analytic signal that Treatment Analysis result measures with judgement.For example, if analytic signal is too faint, may need to reduce dilution gfactor so.In addition, if analytic signal is too strong, instrument may not (may need to use factor D in this case with needed accuracy measurement analytical concentration so
2Further dilute).
Can calculate D with the predetermined maximum level that is used to provide enough accurate results by the upshift signal that compares from analyzer
2As previously mentioned, obtain new dilution gfactor D by the flow velocity 1 of regulating first pump 72
2As a result, owing to can obtain analysis result, therefore can control dilution gfactor in real time from analyzer.
Controller or PC 88 control the flow rate of first pump 72 and second pump 86 respectively.The data that will derive from the instrumental analysis result along link 100 are input in this controller.Respectively by link 102 and 104 controls, first and second pumps.Can be along link 106 control self-actuated samplers and along link 108 gauge tap.Can be with flow rate information or data from these pumps (or any velocimeter; Demonstration) transferring back to controller uses for controller.Therefore, controller may change the dilution gfactor relevant with analyser results (if necessary).For example, too many for Accurate Analysis if the result shows matrix residual in the sample that diluted, so as previously mentioned, controller can reduce the flow rate of first pump, increases dilution gfactor by this.
In case by analysis sample and obtained required result, system 50 just can begin the dilution to new samples, and is as described below.Controller stops first pump 72 and second pump 86 and switch and is manoeuvred into (as mentioned above) in the initial configuration.Restart pump 72 and 86, and next first pump 72 begins thinning agent to be drawn in the 5th pipeline 76 with the slow speed less than flow velocity 3 substantially by switch port A and F and the 4th pipeline 70.Instrument pump 86 extracts a large amount of thinning agents like this and comes diluted sample with the highly diluted factor, and it is drawn in the analyzer instrument with the flow velocity operation of flow velocity 3 or approaching velocity 3 from container 81.Analyzer works on and does not read any reading.When from the 5th pipeline 76, migrating out wherein all samples, the suction that first pump 72 finishes thinning agent.This can be by flow rate F aspirates second fluid or thinning agent 73 is controlled to be scheduled in one section preset time T, wherein
T＞V/F
And V is the shared volume of fluid in switch (between port A and the port F) and the 5th pipeline 76.This helps to guarantee that all remain in the 5th ducted sample and are rushed out and can not pollute the sample that the next one is used to analyze.Can T be minimized by the length (and therefore reducing volume) that reduces the 5th pipeline between switch and the Mixed Zone.
Simultaneously, self-actuated sampler 54 is drawn into new sample in the system, and as previously mentioned, all samples in first and second pipelines (56 and 64) are washed out.
Second or sample suction stage (valve 58 has been switched to the second place) during, first pump 72 is substantially with flow velocity 3 initial periods of work, all thinning agents 73 in the 5th pipeline 76 are by the sample fluid displacement from second pipeline 64.When being full of sample fully in the 5th pipeline, the flow rate of first pump will be reduced to flow velocity 1, and as mentioned above, therefore sample dilution meeting takes place.Can use suitable equation to calculate sample and be full of the needed time of the 5th pipeline fully.
By this way, with the needed accurate flow rate of accurate dilution sample is drawn in the instrument and sample can not pollute or corrode the assembly of first pump 72.In addition, the flush cycle of being used among the present invention has greatly reduced the pollution to system component.
A kind of interchangeable method of judging dilution gfactor can comprise with known concentration level being that sample solution " mixes (spike) " or " adding (lace) " a kind of known substance.This spike is commonly called internal standard compound.It is diluted that the analysis of analyser results is how many samples reduction by known substance content among the described result shows.Certainly, this known substance should be a non-existent material in sample or the thinning agent before adding spike.For example, these known substances may comprise rhodium or indium.
For obtaining point-device dilution factor levels, preferably sample and thinning agent are all mixed.For example, can be mixed with rhodium and concentration level that concentration level is 100/1000000000ths (ppb) be the indium of 10ppb to sample.Thinning agent is not mixed with rhodium, but can be mixed with the indium of 10ppb concentration level.If come diluted sample with (for example) 50 times, rhodium concentration is 2ppb (dilution back) so.The internal standard compound of indium still is the concentration level of 10ppb, and this is because sample and thinning agent all contain the indium of 10ppb.
Yet, if exist in the dilution instability (this instability may be by the bubble in the mixer for example or sample and thinning agent inconsistent mix cause), the value of rhodium concentration can change so.Through under the situation of system, the reading of concentration levels of rhodium may be 1.2ppb at bubble, and the reading of next group is that the reading of 1.99ppb and last batch of is 2.0ppb.This just causes mean value is 1.73ppb, or to cause the error of 50: 1 expection dilution gfactor be 13.5%.Can come by the numerical value of each batch of converting each batch proofreaied and correct; First conversion factor can be the conversion factor that 2/1.2, the second batch conversion factor can be 2/1.99 and the 3rd batch and can be 2/2.0.This can eliminate any error that the concentration of specimens level that measured can take place originally when not noticing the abnormal conditions of dilution gfactor.This to the mixing or use and will allow to surpass 50: 1 dilution of internal standard compound, and do not have the risk that microbubble or melange effect cause data error.
In addition, particularly sample is being drawn in the mixer and the fluid in the mixer is being drawn in the instrument but on one's own initiative thinning agent be not drawn in the mixer (promptly, on the circuit between thinner container and the mixer, there is not pump, therefore under the situation mobile relatively relevant with sample pump and instrument pump of flowing of thinning agent), it is favourable mixing the indium with similar concentration level for thinning agent and sample.When being zero, the dilution gfactor of needs can go wrong.For reaching zero dilution, instrument pump all should be with identical flow rate operation with sample pump.Yet if the operating ratio instrument pump of sample pump is slightly fast, so a part of sample is forced in the thinning agent, thereby pollutes thinning agent.Therefore, sample pump is preferably to move than little about 10% the flow rate of instrument pump flow rate.By this way, sample only is subjected to slight dilution.Detect concentration levels of rhodium and just can solve or judge this little dilution gfactor.
The indium spike also can be used to detect and/or judge contingent any variation in the sample ionization process.Under the situation of ICP-MS, ionization occurs in the plasma torch (torch), and can detect the variation of blowtorch consistance or condition of plasma by the level of detected indium in mass spectrum.This is because indium concentration level 10ppb always, if but detect the indium concentration level less than this concentration, so for example, can proofread and correct the factor that causes the inconsistency in the ion forming process.
The present invention can greatly improve the treatment capacity that realizes instrument of the present invention, and needs the intervention from the operator still less.In addition,, so just can prevent the inlet of host material contamination analysis device, thereby reduce clean this instrument required shut down time if dilution gfactor remains on high relatively level.
The said pump system is a kind of " closure " structure, and it refers to sample and thinning agent all is contained in from switch among the system that exports.By maintenance system closure, top equation is kept during operation.Therefore, guarantee that it is very important that thinning agent and sample can not flow out to prevent that air from entering system during operation.
The pipeline of pumping system 50 or conduit tube component should be made to prevent expanding under what pressure in office or shrink by the appropriate rigidity material.This expansion or contraction are worthless, because it can influence the shared volume of sample of sample, thinning agent and dilution.If expand or the degree of shrinking for can measure or for predictable, so this expansion or contraction are permissible.
Preferably mixer design should be become can be by guaranteeing that in the Mixed Zone of conduit turbulization sample mixes fully with thinning agent.
First pump and second pump should provide continuous substantially the flowing without any pulsation.Can use the independent velocimeter at the front portion that is placed in each pump or rear portion to measure flow rate from each pump, these velocimeters have the suitable backfeed loop to pump controller.Perhaps, can use internal standard compound to measure dilution gfactor.As mentioned above, controller can use the appropriate software program to come the dilution and the conversion from a sample to next sample of robotization sample.Use the controller of suitable software program can comprise Desktop PC and fluid switchgear 58, this Desktop PC has suitable input and output device to monitor and to control these pumps.
The example of the employed sample of embodiments of the invention comprises: the solid of the acid of potable water, waste water, seawater, dilution, urine, blood, spinal fluid, dissolving or gas sample etc.These examples are whole anything but, and any liquid sample of need analyzing is diluted before can be in being implemented pump suction analyzer of the present invention.Certainly, different samples needs the suitable dilution agent, and does not form a part of the present invention for the selection of the thinning agent of given sample.Thinning agent can be deionized water, alcohol etc., but which kind of thinning agent the most suitable be to depend on analyzed sample.
The foregoing description provide a kind of relatively apace and use out of true, uneven flow rate pump (generally very cheap) that sample is drawn into equipment and method in storer or the impact damper.Next (if desired) uses accurate pump to remove from storer or distribute this sample with rate of volume flow relatively slowly, and makes this sample can not enter this accurate pump or pollute the assembly of this pump.By this way, can avoid the cross pollution or the pump corrosion of a plurality of samples.
The those skilled in the art it is contemplated that other embodiments of the invention under the prerequisite that does not deviate from the claim scope.For example, the embodiment that has described uses a plurality of pumps of tandem, but is to use other suction system also to be fine.Equally, thinning agent 80 can be contained in the identical container with 73.In addition, the cleaning solution in the container 62 also can comprise the thinning agent 80 and 73 in the common container.
Claims (43)
1. sample is drawn in the analyzer for the pumping unit of analyzing, comprises:
First pump, described first pump be configured to first flow rate described sample is drawn in the buffer area and
Second pump, described second pump is configured to second flow rate second fluid is drawn in the described buffer area subsequently, so that the described sample of at least a portion is transferred to the analyzer from described buffer area, described second pump can be operated, more accurate control can be subjected to so that described second flow rate is compared described first flow rate.
2. equipment according to claim 1, it is characterized in that, also comprise a mixer, described mixer is arranged on the downstream of described buffer area, and in the upstream that is positioned at the described analyzer on the impact damper outlet conduit, before described mixer is provided in and analyzes with described sample and a mixing diluents to dilute described sample.
3. equipment according to claim 1 and 2 is characterized in that, also comprises the 3rd pump, and described the 3rd pump is configured to be drawn in the described analyzer with the sample that the 3rd flow rate will be diluted.
4. equipment according to claim 3 is characterized in that, with the 4th flow rate described thinning agent is drawn in the described mixer, and described the 4th flow rate is substantially the difference between described the 3rd flow rate and described second flow rate.
5. equipment according to claim 4 is characterized in that, described the 3rd pump is configured to described thinning agent is drawn in the described mixer.
6. according to each described equipment in the aforementioned claim, it is characterized in that described buffer area is configured to have one first port and one second port.
7. equipment according to claim 6, it is characterized in that, described first pump is configured to by described first port described sample be placed described buffer area, and described second pump is configured to by described second port described second fluid be placed described buffer area.
8. according to claim 6 or 7 described equipment, it is characterized in that, also comprise
The fluid flow switch device, it can move between a primary importance and a second place, described fluid flow switch device be provided with like this so that:
(a) when described switchgear is arranged in described primary importance, described buffer area be communicated with the described first pump fluid and
(b) when described switchgear is arranged in the described second place, the described first buffer area port is communicated with described mixer fluid, and the second buffer area port is communicated with the described second pump fluid.
9. equipment according to claim 8 is characterized in that, also comprises a waste solution channel, described waste solution channel be provided with like this so that:
When described switchgear was arranged in described primary importance, described buffer area also was communicated with described waste solution channel fluid.
10. equipment according to claim 8 is characterized in that, described switchgear be provided with like this so that:
When described switchgear was arranged in the described second place, described waste solution channel was communicated with the described first pump fluid, and described first pump is configured to aspirate an irrigation.
11. according to Claim 8,9 or 10 described equipment, it is characterized in that, also comprise:
When described switchgear is arranged in described primary importance, described second pump be arranged on described mixer and be communicated with described outlet conduit fluid between the described buffer area, thereby described second fluid can be drawn in the described outlet conduit, with the displacement described sample fluid or second fluid wherein.
12., it is characterized in that described Mixed Zone comprises two or more input pipes, a mixing portion and an outlet according to claim 2 or 11 described equipment,
First input pipe be configured to described sample fluid be sent to from described buffer area described mixing portion and
Second input pipe is configured to described thinning agent is sent to described mixing portion.
13. according to claim 11 or 12 described equipment, it is characterized in that, also comprise:
When described switchgear is arranged in the described second place,
Described second pump be configured to described second flow rate with the suction of described sample fluid by described Mixed Zone and
Described the 3rd pump is configured to aspirate the sample fluid of diluting with the 3rd flow rate.
14. according to each described equipment in the aforementioned claim, it is characterized in that, also comprise a controller, described controller is used for monitoring during operation and/or regulate at least one pumping unit of described first, second or the 3rd pumping unit, and/or described switchgear.
15. equipment according to claim 14 is characterized in that, described controller is a PC.
16., it is characterized in that described controller is configured to from described analyzer receiving and analyzing data according to claim 14 or 15 described equipment.
17. according to claim 13 and 16 described equipment, it is characterized in that, described third speed substantially more than or equal to described second speed and
Wherein said controller is configured to respond the analysis data that received and regulates described first and/or third speed.
18. equipment according to claim 17 is characterized in that, described controller is configured to regulate in real time described flow rate.
19. equipment according to claim 1 is characterized in that, described analyzer is a mass spectrometer or an inductively coupled plasma mass spectrometry instrument.
20. equipment according to claim 1 is characterized in that, described second pumping unit comprises a piston pump.
21. an analyzer that is used for the analyzing samples fluid, it comprises according to each described suction system in the aforementioned claim.
22. analyzer according to claim 21 is characterized in that, described analyzer is a mass spectrometer or an inductively coupled plasma mass spectrometry instrument.
23. one kind is used extracting device that sample fluid is drawn in the analytical instrument for the method for analyzing, described extracting device comprises:
The buffer area of the described sample fluid of interim storage, described buffer area is provided with at least two ports,
Use first pumping unit by first port described sample fluid to be placed described buffer area with first flow rate, and
Described method comprises:
Use second pumping unit with second flow rate by second port with second fluid extraction in the described buffer area that is filled to small part, by this described sample fluid in the described buffer area is transferred in the described analyzer,
Described whereby second pumping unit is compared described first pumping unit can be subjected to more accurate control.
24. method according to claim 23 is characterized in that, described equipment also comprises:
The fluid flow switch device, it can move between a primary importance and a second place, described fluid flow switch device be provided with like this so that:
(a) when described switchgear is arranged in described primary importance, described buffer area be communicated with the described first pump fluid and
(b) when described switchgear is arranged in the described second place, the described first buffer area port is communicated with described mixer fluid, and the second buffer area port is communicated with the described second pump fluid;
Described method also comprises:
When described fluid flow switch device is arranged in described primary importance, use described first pump that described sample is drawn in the described impact damper,
With described fluid flow switch device switch to the described second place and
Use described second pump that described second fluid is drawn in the described buffer area, so that replace the described sample in the described buffer area.
25. method according to claim 24 is characterised in that, described equipment also comprises a waste solution channel, and described waste solution channel is provided with like this, so that when described switchgear was arranged in described primary importance, a buffer area port was communicated with the waste solution channel fluid,
Described method also comprises:
Fluid excessive in the described buffer area is drawn in the described waste solution channel.
26. method according to claim 25 is characterized in that, also comprises:
When described switchgear was arranged in the described second place, described waste solution channel was communicated with the described first pump fluid, and described first pump aspirates an irrigation.
27., be characterised in that described method also comprises according to each described method in the claim 24 to 26:
When described switchgear is arranged in described primary importance, described second pump be communicated with described outlet conduit fluid and
Described second pump is drawn into described second fluid in the described outlet conduit, so that the displacement described sample fluid or second fluid wherein.
28., be characterised in that described equipment also comprises according to each described method in the claim 24 to 27:
The Mixed Zone, its be used for described sample fluid and a mixing diluents and
The 3rd pumping unit, its sample fluid that will dilute is drawn into described analyzer from described Mixed Zone,
Wherein, described Mixed Zone is set between described outlet conduit and the described analyzer;
Described method also comprises:
When described switchgear is arranged in the described second place,
Described second pumping unit is drawn into sample fluid in the described buffer area with second flow rate,
Described the 3rd pumping unit with the 3rd flow rate aspirate described dilution sample fluid and
Described the 3rd pumping unit aspirates described thinning agent with the 4th flow rate, and described the 4th flow rate equals the difference of described the 3rd flow rate and described second flow rate substantially.
29. according to each described method in the claim 24 to 28, it is characterized in that described equipment also comprises a controller, described monitoring control devices and/or regulate at least one pumping unit in described first, second or the 3rd pumping unit, and/or described switchgear.
30. method according to claim 29 is characterized in that, described controller receives the analysis data from described analyzer.
31., it is characterized in that described third speed is equal to or greater than described second speed substantially according to claim 28 and 30 described methods, and
Analysis data that the response of wherein said controller is received and regulate described first and/or third speed.
32. method according to claim 31 is characterized in that, described controller is regulated described flow rate in real time.
33. the method for dilution one a sample fluid, it uses according to each described equipment in the claim 1 to 22 with according to each described method in the claim 23 to 32.
34. a computer program when it moves on a computer, is carried out according to each described method in the claim 23 to 33.
35. an electron carrier device has been stored computer program according to claim 33 on it.
36. a method that prevents that first pumping unit from being polluted by a sample, described method comprises:
Use one second pump that described sample is placed a zone line,
By using described first pumping unit that one second fluid is drawn in the described zone line, and described sample is migrated out from described zone line.
37. dilution one a sample fluid is for the dilution system of analyzing, it comprises:
The buffer area, it is used to store described sample fluid and is provided with an input end and an output terminal,
First pumping unit, it is used for by described input end described sample fluid being drawn into the sample fluid buffer area,
Second pumping unit, it is used for by described output terminal one second fluid being drawn into described buffer area,
Outlet conduit, its fluid that is configured to supply described sample fluid and/or flow to described analyzer flows
The Mixed Zone, it is a described sample fluid and a mixing diluents,
The 3rd pumping unit, its sample fluid that is used for diluting be drawn into from described Mixed Zone described analyzer and
The fluid flow switch device, it can move between a primary importance and a second place, described fluid flow switch device be provided with like this so that:
When described switchgear was arranged in described primary importance, described buffer area input end was communicated with described first pump, and described sample fluid can be sucked in the described buffer area and
When described switchgear is arranged in the described second place, described buffer area input end is communicated with described outlet conduit, and described buffer area output terminal is communicated with described second pump, so that described second fluid can be sucked in the described buffer area, replacing the described sample in the described buffer area, and wherein said Mixed Zone is arranged between described outlet conduit and the described analyzer.
38. one kind is used dilution system diluted sample fluid for the method for analyzing, this dilution system comprises:
The buffer area, it is used to store described sample fluid and is provided with an input end and an output terminal,
Outlet conduit, it is configured to flow to described analyzer for the described sample fluid and/or second fluid,
The Mixed Zone, its be used for described sample fluid and a mixing diluents and
The 3rd pumping unit, its sample fluid that is configured to dilute is drawn into described analyzer from described Mixed Zone, described Mixed Zone be arranged between described outlet conduit and the described analyzer and
The fluid flow switch device, it can move between a primary importance and a second place, described fluid flow switch device be provided with like this so that: when described switchgear is arranged in described primary importance, described buffer area input end is communicated with first pump, and when described switchgear is arranged in the described second place, described buffer area input end is communicated with described outlet conduit, and described buffer area output terminal is communicated with second pump;
Described method comprises:
When described switchgear is positioned at described primary importance place, use described first pumping unit described sample fluid to be drawn in the described sample fluid buffer area by described input end,
Described switchgear is switched to described second place place,
By described output terminal one fluid is drawn in the described buffer area, by this described sample fluid in the described buffer area is transferred in the described outlet conduit,
When described switchgear was arranged in the described second place, described second pumping unit was drawn into described second fluid in the described buffer area with first flow rate, so that described sample fluid is passed described Mixed Zone with described first fluid speed,
The sample fluid that described the 3rd pumping unit diluted with the 3rd flow rate suction and
Described the 3rd pumping unit aspirates described thinning agent with second flow rate, and described second flow rate equals the difference of described the 3rd flow rate and described first flow rate substantially.
39. one kind is used first pump to aspirate a fluid sample by the method for a diluter with the fluid sample of the dilution of analyzing described diluter downstream, described first pump and described fluid sample are isolated, and described method comprises:
Use one second pump that described fluid sample is placed a zone line, described zone line has first and second ports, and fluid can flow by described port,
Use described first pump one second fluid to be introduced in the described zone line by described second port, so as to the described fluid sample of at least a portion is migrated out from described zone line by described first port, described first port is communicated with described diluter fluid, so that the described fluid sample of this at least a portion is transferred to the described diluter from described zone line.
40. according to each described method in the claim 23 to 39, it is characterized in that, also comprise:
One internal standard compound is placed described sample, described internal standard compound comprise a concentration known predetermined substance and
Compare by concentration known, and determine the dilution gfactor of described sample internal standard compound described in the sample of the detected concentration of described internal standard compound and undiluted mistake.
41., it is characterized in that one second internal standard compound is placed described sample and described thinning agent with the second identical concentration level, and described second internal standard compound comprises second predetermined substance of a concentration known according to the described method of claim 40.
42. according to claim 40 or 41 described methods, it is characterized in that, also comprise:
According to judging described dilution gfactor by the amount of detected described first internal standard compound of described analyzer,
Dilution gfactor by the dilution gfactor that will be judged and an expection compares, and judge a correction factor and
Use described correction factor to come correction analysis device data.
43. equipment according to claim 1 is characterized in that, described sample and/or described thinning agent contain an internal standard compound, and described internal standard compound comprises the known substance of a scheduled volume, and
By comparing, calculate in order to dilute the dilution gfactor of described sample by the amount of the detected described internal standard compound of described analyzer and the amount of the internal standard compound in described sample or the thinning agent.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| GBGB0218949.6A GB0218949D0 (en) | 2002-08-14 | 2002-08-14 | Pumping and diluting a sample for analysis |
| GB0218949.6 | 2002-08-14 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1675530A true CN1675530A (en) | 2005-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN03819412.0A Pending CN1675530A (en) | 2002-08-14 | 2003-08-14 | Method and apparatus for pumping and diluting a sample |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20060104827A1 (en) |
| EP (1) | EP1540305A1 (en) |
| JP (1) | JP2005535893A (en) |
| CN (1) | CN1675530A (en) |
| AU (1) | AU2003255792A1 (en) |
| CA (1) | CA2497648A1 (en) |
| GB (1) | GB0218949D0 (en) |
| WO (1) | WO2004017045A1 (en) |
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- 2003-08-14 AU AU2003255792A patent/AU2003255792A1/en not_active Abandoned
- 2003-08-14 EP EP03787896A patent/EP1540305A1/en not_active Withdrawn
- 2003-08-14 WO PCT/GB2003/003564 patent/WO2004017045A1/en active Application Filing
- 2003-08-14 US US10/524,706 patent/US20060104827A1/en not_active Abandoned
- 2003-08-14 CN CN03819412.0A patent/CN1675530A/en active Pending
- 2003-08-14 JP JP2004528674A patent/JP2005535893A/en active Pending
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| CN103091152A (en) * | 2013-02-21 | 2013-05-08 | 广州伊创仪器有限公司 | Intelligent dilution system and intelligent dilution method for on-line analyzer |
| CN103852369A (en) * | 2014-03-24 | 2014-06-11 | 深圳市清时捷科技有限公司 | Diluting device and method |
| CN103852369B (en) * | 2014-03-24 | 2017-05-17 | 深圳市清时捷科技有限公司 | Diluting device and method |
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| CN109313168B (en) * | 2016-05-05 | 2022-05-27 | 沃特世科技公司 | Method and apparatus for injecting chromatographic samples |
| CN109313168A (en) * | 2016-05-05 | 2019-02-05 | 沃特世科技公司 | Method and apparatus for injecting chromatographic sample |
| CN111433584A (en) * | 2017-11-22 | 2020-07-17 | 拜克门寇尔特公司 | Diluent preparation module and unit |
| CN111433584B (en) * | 2017-11-22 | 2023-10-31 | 拜克门寇尔特公司 | Diluent preparation module and unit |
| US11940459B2 (en) | 2017-11-22 | 2024-03-26 | Beckman Coulter, Inc. | Diluent preparation module |
| CN112955750A (en) * | 2018-12-06 | 2021-06-11 | 株式会社日立高新技术 | Automatic analyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1540305A1 (en) | 2005-06-15 |
| GB0218949D0 (en) | 2002-09-25 |
| CA2497648A1 (en) | 2004-02-26 |
| WO2004017045A1 (en) | 2004-02-26 |
| US20060104827A1 (en) | 2006-05-18 |
| AU2003255792A1 (en) | 2004-03-03 |
| JP2005535893A (en) | 2005-11-24 |
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